岛津原子吸收应用英文手册(元素的测量条件火焰法)03_Measuring_Conditions_by_Element_Flame_AA.docx
ATOMIC ABSORPTION SPECTROPHOTOMETRYCOOKBOOKSection 3Measuring Conditions by Element of Flame AtomicAbsorption SpectrophotometryAtomic Absorption Spectrophotometry CookbookSection 3CONTENTS6. Measuring Conditions by Element ofFlame Atomic Absorption Spectrophotometry16.1 Measuring concentration16.2 Measuring conditions 16.3 Background correction methodand interference16.4 Measuring conditions by element11) Silver(Ag) 22) Aluminum(AZ) 33) Arsenic(As) 44) Gold(Au) 55) Boron(B) 66) Barium(Ba) 77) Beryllium(Be) 88) Bismuth(Bi) 99) Calcium(Ca)I 1010) Calcium(Ca) II 1111) Cadmium(Cd) 1212) Cobalt(Co) 1313) Chromium(Cr) 1414) Cesium(Cs) 1515) Copper(Cu) 1616) Iron(Fe) 1717) Gallium(Ga) 1818) Germanium(Ge) 1919) Potassium(K) 2020) Lithium(Li) 2121) Magnesium(Mg) 2222) Manganese(Mn) 2323) Molybdenum(Mo) 2424) Sodium(Na) 2525) Nickel(Ni) 2626) Lead(Pb)I 2727) Lead(Pb) II 2828) Palladium(Pd) 2929) Platinum(Pt) 3030) Rubidium(Rb) 3131) Rhodium(Rh) 3232) Antimony(Sb) 3333) Selenium(Se) 3434) Silicon(Si) 3535) Tin(Sn)I 3636) Tin(Sn) II 3737) Tin(Sn) III 3838) Tin(Sn) IV 3939) Strontium(Sr) 4040) Tellurium(Te) 4141) Titanium(Ti) 4242) Thallium(T) 4343) Vanadium(V) 4444) Zinc(Zn) 456.Measuring Conditions by Element ofFlame Atomic Absorption Spectrophotometry6.1 Measuring concentrationThe solution prepared on the basis of the standard sample preparation method in the cookbook section 2 - 3 is used to make the calibration curve in the standard concentration range. Because absorbance is 0.044 to 0.3 in the cookbook section 2-4, the upper and lower limits of the calibration line are obtained from the above data to determine the practical measuring concentration range.The measuring concentration range of an actual sample may differ from the data, due to a co-existent matter. Sensitivity of an organic solvent type sample is raised by two or three times.To make a measurement of higher concentrations, the burner must be tilted (Cookbook Section 2 - 4.3) or another analysis line must be used. (Cookbook Section 1 - 2.1).6.2 Measuring conditionsIn the AA-6400 or the AA-6500, the analysis conditions stored can be used. Because there is a slight difference between instruments, it may be better to change the mixing ratio of oxidant and fuel gas in accordance with the cookbook(section 1 - 2.2). This allows data of high sensitivity and good repeatability to be obtained.However, these conditions are for a water solution sample.Therefore, oxidant flow, fuel gas flow, burner height and other conditions must be changed when an organic solvent type sample is measured. Refer to the operating instructions of the atomic absorption spectrophotometer for selection of the optimum conditions.In the cases of calcium, lead, and tin as the target elements, two or more flame conditions and analysis wavelengths are indicated by a I, II, III, or IV.6.3 Background correction method and interferenceConcerning elements for which the selfreversal hollow cathode lamp is available, background correction is done by the D2 lamp method and the selfreversal method. Their results are shown respectively as BGD-D2 mode and BGC-SR mode. In case of BGC-SR9 sensitivity drop occurs due to its principle reason. The BGC-D2 is recommended as a rule when background correction is done.But, in the case of a sample which has the background absorption above 0.5Abs or has any spectral interface, or in the case its analysis line is in a longer wavelength range for which the D2 lamp cannot be used, BGC-SR mode is desirable.Data in this section shows information on interference.In measuring an actual sample, confirmation of interference is necessary. Refer to the cookbook section 2 - 5 for interference in the atomic absorption method.6.4 Measuring conditions by elementStandard substance and standard solution preparation methodRefer to Section 2 - 3 for the Standard solution preparation methodMeasuring conditions and Calibration curve Measuring conditionsCurrent; 10 mA0 mAWave length Slit width Lighting mode;328.1 nm;0.5 nm;BGC-D2;10 mA/400 mA;328.1 nm;0.5 nm;BGC-SRBurner height Burner angle Fuel gas flow Type of oxidant;7 mm;Odeg;2.2 /min;air Calibration curve in BGCD2 modeSTD.CONC.ABS.No.(PPm)328.Inm10.50000.096721.00000.189232.00000.371643.00000.547054.00000.7179ABS.80 0CONC.(PPln)ABS=K2*C2+K1*C+KOKo= 0.0000, KI= 0.1923, K2= -0.0032 Calibration curve in BGC-SR modeSTD.CONC.ABS.No.(pp)328.Inm10.50000.064521.00000.129732.00000.259643.00000.390354.00000.521500CONCJppm)5.ABS=K2*C2+K1*C+KOKo= 0.0000, Kl= 0.1293, K2= 0.0003InterferenceChemic